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Method for preparing epoxy resin by utilizing lignin

A technology of epoxy resin and lignin, which is applied in the field of preparing epoxy resin by using lignin, can solve the problems of low product performance and inability to realize commercial utilization of the preparation method, and achieve good commercial application prospects, small reaction condition restrictions, highly operable effect

Inactive Publication Date: 2015-09-09
ANHUI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, the existing method of using lignin to prepare epoxy resin cannot be truly commercialized due to the limitation of its preparation method and the product performance is far lower than that of the traditional process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The method utilizing lignin to prepare epoxy resin comprises the following steps:

[0024] (1) Pretreatment of lignin

[0025] The alkali lignin was crushed to 80 mesh, then dried to constant weight at 109°C, and then fully dissolved in a concentration of 1.2mol. L -1 in the NaOH solution, and then filtered, and then with a concentration of 1.2mol L -1 The pH value of the obtained filtrate was adjusted to 2 with the HCl solution, and finally the filtrate was left to stand (2h), solid-liquid separation treatment, and then the obtained solid was washed to neutral, and then vacuum-dried at 40°C;

[0026] (2) Oxidative modification of lignin

[0027] Get 2 parts by weight of pretreated lignin and 62 parts by weight of 30% H 2 o 2 The solution was added to 30 parts by weight of ionic liquid [BMIm]Cl with a mass fraction of 99.2%, the pH value was adjusted to 8 by NaOH solution, and then the oxidation reaction was carried out at 90° C. for 2 h, and finally the mixture ob...

Embodiment 2

[0032] The method utilizing lignin to prepare epoxy resin comprises the following steps:

[0033] (1) Pretreatment of lignin

[0034] The alkali lignin was crushed to 90 mesh, then dried to constant weight at 90°C, and then fully dissolved in a concentration of 0.5mol. L -1 in the NaOH solution, and then filtered, and then with a concentration of 0.5mol L -1 HCl solution to adjust the pH value of the obtained filtrate to 2.5, and finally the filtrate was left to stand (2h), solid-liquid separation treatment, and then the obtained solid was washed to neutral, and then vacuum-dried at 40°C;

[0035] (2) Oxidative modification of lignin

[0036] Take 1 weight part of pretreated lignin and 35 parts by weight of 30% H 2 o 2 The solution was added to 40 parts by weight of ionic liquid [BMIm]Cl with a mass fraction of 99.5%, the pH value was adjusted to 9 by NaOH solution, and then oxidized at 50° C. for 4 h, and finally the mixture obtained from the oxidized reaction was static...

Embodiment 3

[0041] The method utilizing lignin to prepare epoxy resin comprises the following steps:

[0042] (1) Pretreatment of lignin

[0043] The alkali lignin was crushed to 100 mesh, then dried to constant weight at 100°C, and then fully dissolved in a concentration of 2mol. L -1 in the NaOH solution, and then filtered, and then with a concentration of 2mol L -1 The pH value of the obtained filtrate was adjusted to 3 with the HCl solution, and finally the filtrate was left to stand (2h), solid-liquid separation treatment, and then the obtained solid was washed to neutral, and then vacuum-dried at 40°C;

[0044] (2) Oxidative modification of lignin

[0045] Get 3 parts by weight of pretreated lignin and 90 parts by weight of 30% H 2 o 2 The solution was added to 50 parts by weight of ionic liquid [BMIm]Cl with a mass fraction of 99.5%, the pH value was adjusted to 10 by NaOH solution, and then the oxidation reaction was carried out at 70° C. for 3 h, and finally the mixture obta...

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Abstract

The invention relates to a method for preparing epoxy resin by utilizing lignin. The method for preparing epoxy resin by utilizing lignin comprises the following steps: (1) smashing lignin, and then removing inorganic salt impurities in lignin; (2) adding pretreated lignin and H2O2 solution into ionic liquid [BMIm]Cl, regulating the pH value to be 8-10, then carrying out oxidation reaction for 2-4 hours at the temperature of 50-90 DEG C, and finally carrying out standing and solid-liquid separation on the mixture obtained through the oxidation reaction, wherein the obtained solid matter is namely oxidized and modified lignin; and (3) adding 35-60 parts by weight of 10-20% NaOH solution and 45-90 parts by weight of epoxy chloropropane into the oxidized and modified lignin, then carrying out epoxidation reaction for 2-5 hours at the temperature of 70-100 DEG C, and finally standing and removing unreacted raw materials from the mixture obtained through the epoxidation reaction, so that the epoxy resin is obtained. The method for preparing epoxy resin by utilizing lignin is economic and environmental-friendly and is strong in operability, and the obtained epoxy resin product has good performance and has a very good commercial application prospect.

Description

technical field [0001] The invention relates to the field of epoxy resin synthesis, in particular to a method for preparing epoxy resin from lignin. Background technique [0002] Lignin is the second largest renewable resource next to cellulose in nature, with an annual cost of 5×10 10 It can be regenerated at a speed of t and is an organic raw material with great industrial value. In cellulose-related industries such as plant hydrolysis and pulp and paper industry, lignin is usually produced in large quantities in the form of by-products, such as about 20-30% lignin in papermaking black liquor. But so far, more than 95% of the separated lignin recovery is concentrated and then burned. On the one hand, it causes a great waste of resources, and on the other hand, the discharge of lignin-containing industrial wastewater will also cause serious adverse effects on the environment. Effective utilization of lignin is of positive significance to my country's environmental protect...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/02C08H7/00
Inventor 陈明强刘珂杨忠连刘少敏
Owner ANHUI UNIV OF SCI & TECH
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